Two-way, unfolded three-way and three-mode partial least squares calibration of diode array HPLC chromatograms for the quantitation of low-level pharmaceutical impurities

Abstract A series of two-way diode array chromatograms were recorded at 0.1–0.5% and 1–5% of 3-hydroxypyridine impurity co-eluting with 2-hydroxypyridine, recorded at pH 4.9 (good resolution) and 5.0 (poor resolution). Four methods for PLS calibration, namely, using summed spectral profiles, summed elution profiles, unfolded three-way PLS and true three-way PLS were applied to the datasets, both using autopredictions and cross-validation. It was found that it was possible to accurately quantify low levels of impurities. Three-way methods often performed worse than two-way methods using the summed spectral profile probably due to irreproducibility of elution times.

[1]  S. Wold,et al.  The Collinearity Problem in Linear Regression. The Partial Least Squares (PLS) Approach to Generalized Inverses , 1984 .

[2]  R. Brereton,et al.  Multivariate calibration of chlorophyll a using partial least squares and electronic absorption spectroscopy , 1996 .

[3]  Tormod Næs,et al.  Multivariate calibration. II. Chemometric methods , 1984 .

[4]  Katta G. Murty,et al.  On KΔ , 1986, Discret. Appl. Math..

[5]  R. Brereton,et al.  Calibration of Gas Chromatography-Mass Spectrometry of Two-component Mixtures Using Univariate Regression and Two- and Three-Way Partial Least Squares , 1997 .

[6]  Multivariate detection limits for selected ion monitoring gas chromatography — mass spectrometry , 1988 .

[7]  D. Kell,et al.  Improving the interpretation of multivariate and rule induction models by using a peak parameter representation , 1997 .

[8]  R. Brereton,et al.  Multivariate calibration on designed mixtures of four pharmaceuticals , 1998 .

[9]  B. Kowalski,et al.  Partial least-squares regression: a tutorial , 1986 .

[10]  R. Brereton,et al.  Chemometric analysis of high performance liquid chromatography-diode array detection-electrospray mass spectrometry of 2- and 3-hydroxypyridine. , 1998, The Analyst.

[11]  Age K. Smilde,et al.  Three-way analyses problems and prospects , 1992 .

[12]  J. T. Clerc,et al.  Trends in analytical chemistry , 1980 .

[13]  R. Brereton,et al.  Partial least-squares calibration of two-way diode-array high-performance liquid chromatograms: influence of calibration design, noise and peak separation , 1998 .

[14]  Paul Geladi,et al.  Analysis of multi-way (multi-mode) data , 1989 .

[15]  Svante Wold,et al.  Partial least-squares method for spectrofluorimetric analysis of mixtures of humic acid and lignin sulfonate , 1983 .

[16]  S. A. bano C. D. nn W. I. i Wold,et al.  Pattern recognition: finding and using regularities in multivariate data Food research, how to relate sets of measurements or observations to each other , 1983 .

[17]  T. Ryan.  HPLC Impurity Profile Analyses of Pharmaceutical Substances Using UV Photodiode Array DEtection , 1998 .

[18]  R. Brereton,et al.  Application of partial least squares calibration to measurements of polycyclic aromatic hydrocarbons in coal tar pitch volatiles , 1996 .

[19]  S. Wold,et al.  Multi‐way principal components‐and PLS‐analysis , 1987 .

[20]  G. G. Stokes.  "J." , 1890, The New Yale Book of Quotations.

[21]  Lars St»hle,et al.  Aspects of the analysis of three-way data , 1989 .

[22]  R. Bro.  Multiway calibration. Multilinear PLS , 1996 .

[23]  S. Görög,et al.  Estimation of impurity profiles of drugs and related materials. Part 9: HPLC investigation of flumecinol. , 1992, Journal of pharmaceutical and biomedical analysis.

[24]  Paul Geladi,et al.  An example of 2-block predictive partial least-squares regression with simulated data , 1986 .